CN109809502A - A method of nickel sulfate is produced using electro deposited nickel anolyte - Google Patents
A method of nickel sulfate is produced using electro deposited nickel anolyte Download PDFInfo
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- CN109809502A CN109809502A CN201910238948.3A CN201910238948A CN109809502A CN 109809502 A CN109809502 A CN 109809502A CN 201910238948 A CN201910238948 A CN 201910238948A CN 109809502 A CN109809502 A CN 109809502A
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- nickel
- nickel sulfate
- sulfate
- anolyte
- sulfuric acid
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Abstract
The invention discloses a kind of methods using electro deposited nickel anolyte production nickel sulfate, this method is to contain nickel sulfate and certain acidity and the low feature of impurity content using electro deposited nickel anolyte, nitration mixture slot is proportionally added into sulfuric acid, and nickel-contained mixed acid solution is made, pure water is added simultaneously, nickel bead or nickel powder is added after adjusting the sulfuric acid concentration in nickel-contained mixed acid solution, nickel bead or nickel powder are dissolved in generation nickel sulfate rich solution in sulfuric acid, by nickel sulfate rich solution filtering and impurity removing, crystallisation by cooling, centrifuge separation, nickel sulfate product is obtained after drying, simple process, production cost is low, realize the recycling of nickel and acid in electro deposited nickel anolyte, the waste of resource is not will cause.
Description
Technical field
The invention belongs to chemical metallurgies, technical field of wet metallurgy, and in particular to a kind of to be produced using electro deposited nickel anolyte
The method of nickel sulfate.
Background technique
Nickel sulfate reparation technology is different because of raw material and product purpose difference, and the reparation technology generallyd use at present is: will be electric
Nickel or carbonyl nickel sulfuric acid dissolution, rich nickel solution evaporative crystallization form.Its advantage is that process flow is short, product quality is high, disadvantage
It is that electric nickel price is higher, high production cost.
And electricity Nie manufacturer generallys use leaching-insoluble anode diaphragm electrolysis production technology, electrolytic deposition process generates anode
Liquid, which returns, leaches process as acid solution progress ingredient.Electrolytic deposition process anode uses insoluble anode, allows in electrolyte and is intended to extract
Metal deposit and be precipitated on cathode, thus achieve the purpose that extract metal.In the catholyte of nickel electrowinning, in addition to containing H+
Outside, the metal ion often containing objectionable impurities such as a small amount of copper, iron, cobalt, zinc, although the content of these foreign ions is very low, mark
Collimator electrode current potential is compared with Ni2+Positive Cu2+、Pb2+Plasma is restored prior to nickel ion and is precipitated, therefore the anolyte that electrodeposition generates passes through
Reach certain purification after electrolysis；Traditional method is that electrodeposition is generated to process before anolyte returns to carry out ingredient, causes to waste.It is public
A kind of method for producing electro deposited nickel of number patent disclosure for being CN105441974B is accused, the anolyte that electrodeposition is generated is through extraordinary yin
So that pH is reached 2.5-3.5 after ion diffusion dialysis, enters Winning cell production Ni9996 electro deposited nickel as electrodeposition catholyte.The work
Though skill recycles and produce Ni9996 electro deposited nickel, process carries out ingredient before secondary anode liquid still returns.This secondary anode liquid
By electrodeposition twice, double purification is obtained, chemical component impurity content is lower than initial catholyte, and process carries out ingredient before returning,
Waste is serious.
Summary of the invention
The purpose of the present invention is to solve the technical problems existing in the prior art, a kind of simple process, production are provided
The method using electro deposited nickel anolyte production nickel sulfate that is at low cost, will not resulting in waste of resources.
In order to achieve the above object, the invention adopts the following technical scheme: a kind of produce sulfuric acid using electro deposited nickel anolyte
The method of nickel, method includes the following steps:
A, nitration mixture slot is added according to volume ratio 1:1 in electro deposited nickel anolyte and sulfuric acid and nickel-contained mixed acid solution is made；
B, pure water is added in nickel-contained mixed acid solution, adjusting sulfuric acid concentration in nickel-contained mixed acid solution is 1-1.5M；
C, the nickel-contained mixed acid solution adjusted and nickel bead are added in reactor, or nickel-contained mixed acid solution and carbonyl that will adjust
Nickel powder is added in nickel powder dissolving tank；
D, adjusting the reaction temperature in reactor or nickel powder dissolving tank is 70 DEG C -85 DEG C, and the reaction time is 6-8 hours, and reaction is eventually
Point pH value is 1.5-4.0, and nickel bead or carbonyl nickel powder are dissolved in generation nickel sulfate rich solution, sulfuric acid in the sulfuric acid in nickel-contained mixed acid solution
Nickel sulfate content is 298-356 g/L in nickel rich solution；
E, by nickel sulfate rich solution filtering and impurity removing, filtered filtrate enters crystallization tank crystallisation by cooling and obtains nickel sulfate magma；
F, wet nickel sulfate hexahydrate crystal is obtained after being centrifugated nickel sulfate magma by centrifugal separator；
G, wet nickel sulfate hexahydrate crystal is sent into drier and is dried, obtain nickel sulfate product.
Further, the concentration of sulfuric acid is 93% in the step A.
Further, crystallization temperature is 15 DEG C -25 DEG C in the step E.
Further, the reactor or nickel in nickel sulfate mother liquor return step C obtained after being centrifugated in the step F
Powder dissolving tank recycles.
Further, wet nickel sulfate hexahydrate crystal is sent into fluidized bed dryer in the step G by auger conveyor and is dried,
Drying temperature is 35 DEG C -45 DEG C.
The present invention has the advantages that the present invention using electro deposited nickel anolyte production nickel sulfate compared with the prior art
Method is to contain nickel sulfate and certain acidity and the low feature of impurity content using electro deposited nickel anolyte, is added in proportion with sulfuric acid
Enter nitration mixture slot and nickel-contained mixed acid solution is made, while pure water is added, nickel bead is added after adjusting the sulfuric acid concentration in nickel-contained mixed acid solution
Or nickel powder, nickel bead or nickel powder are dissolved in generation nickel sulfate rich solution in sulfuric acid, by nickel sulfate rich solution filtering and impurity removing, crystallisation by cooling, from
Nickel sulfate product is obtained after heart separation, drying, simple process, production cost is low, realizes nickel and acid in electro deposited nickel anolyte
It recycles, not will cause the waste of resource.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1
Free sulfuric acid content 20-35g/L, Ni in certain electro deposited nickel anolyte2+>=47g/L, Co2+﹤ 0.003g/L, Cu2+﹤
0.002g/L、Fe2+﹤ 0.001g/L, Pb2+﹤ 0.0004g/L.
A, by electro deposited nickel anolyte and mass concentration be 93% sulfuric acid according to volume ratio 1:1 be added nitration mixture slot be made it is nickeliferous
Mixed acid solution.
B, pure water is added in nickel-contained mixed acid solution, adjusting sulfuric acid concentration in nickel-contained mixed acid solution is 1M.
C, the nickel-contained mixed acid solution adjusted and nickel bead are added in reactor, nickel bead ingredient is Ni >=99.97%, Co ﹤
0.02%, C ﹤ 0.005%, Cu ﹤ 0.002%, Fe ﹤ 0.002%, Pb2+ ﹤ 0.0008%；Or the nickel-contained mixed acid solution and carbonyl that will be adjusted
Base nickel powder is added in nickel powder dissolving tank.
D, adjusting the reaction temperature in reactor or nickel powder dissolving tank is 70 DEG C, and the reaction time is 8 hours, reaction end pH
Value is 1.5, and nickel bead or carbonyl nickel powder, which are dissolved in the sulfuric acid in nickel-contained mixed acid solution, generates nickel sulfate rich solution, in nickel sulfate rich solution
Nickel sulfate content is 298 g/L.
E, by nickel sulfate rich solution filtering and impurity removing, filtered filtrate enters crystallization tank crystallisation by cooling, and crystallization temperature is 15 DEG C,
Nickel sulfate magma is obtained after crystallisation by cooling.
F, wet nickel sulfate hexahydrate crystal is obtained after being centrifugated nickel sulfate magma by centrifugal separator, is obtained after centrifuge separation
Nickel sulfate mother liquor enter mother liquor tank, as in mother liquor return step C reactor or nickel powder dissolving tank recycle.
G, wet nickel sulfate hexahydrate crystal is sent into fluidized bed dryer by auger conveyor and is dried, drying temperature is 35 DEG C, is dried
Nickel sulfate product is obtained after dry, is sent into baling line and is packed.
Nickel sulfate product testing result is as follows:
Embodiment 2
Free sulfuric acid content 20-35g/L, Ni in certain electro deposited nickel anolyte2+>=47g/L, Co2+﹤ 0.003g/L, Cu2+﹤
0.002g/L、Fe2+﹤ 0.001g/L, Pb2+﹤ 0.0004g/L.
A, by electro deposited nickel anolyte and mass concentration be 93% sulfuric acid according to volume ratio 1:1 be added nitration mixture slot be made it is nickeliferous
Mixed acid solution.
B, pure water is added in nickel-contained mixed acid solution, adjusting sulfuric acid concentration in nickel-contained mixed acid solution is 1.5M.
C, the nickel-contained mixed acid solution adjusted and nickel bead are added in reactor, nickel bead ingredient is Ni >=99.97%, Co ﹤
0.02%, C ﹤ 0.005%, Cu ﹤ 0.002%, Fe ﹤ 0.002%, Pb2+ ﹤ 0.0008%；Or the nickel-contained mixed acid solution and carbonyl that will be adjusted
Base nickel powder is added in nickel powder dissolving tank.
D, adjusting the reaction temperature in reactor or nickel powder dissolving tank is 85 DEG C, and the reaction time is 6 hours, reaction end pH
Value is 4.0, and nickel bead or carbonyl nickel powder, which are dissolved in the sulfuric acid in nickel-contained mixed acid solution, generates nickel sulfate rich solution, in nickel sulfate rich solution
Nickel sulfate content is 302 g/L.
E, by nickel sulfate rich solution filtering and impurity removing, filtered filtrate enters crystallization tank crystallisation by cooling, and crystallization temperature is 25 DEG C,
Nickel sulfate magma is obtained after crystallisation by cooling.
F, wet nickel sulfate hexahydrate crystal is obtained after being centrifugated nickel sulfate magma by centrifugal separator, is obtained after centrifuge separation
Nickel sulfate mother liquor enter mother liquor tank, as in mother liquor return step C reactor or nickel powder dissolving tank recycle.
G, wet nickel sulfate hexahydrate crystal is sent into fluidized bed dryer by auger conveyor and is dried, drying temperature is 45 DEG C, is dried
Nickel sulfate product is obtained after dry, is sent into baling line and is packed.
Nickel sulfate product testing result is as follows:
Embodiment 3
Free sulfuric acid content 20-35g/L, Ni in certain electro deposited nickel anolyte2+>=47g/L, Co2+﹤ 0.003g/L, Cu2+﹤
0.002g/L、Fe2+﹤ 0.001g/L, Pb2+﹤ 0.0004g/L.
A, by electro deposited nickel anolyte and mass concentration be 93% sulfuric acid according to volume ratio 1:1 be added nitration mixture slot be made it is nickeliferous
Mixed acid solution.
B, pure water is added in nickel-contained mixed acid solution, adjusting sulfuric acid concentration in nickel-contained mixed acid solution is 1.2M.
C, the nickel-contained mixed acid solution adjusted and nickel bead are added in reactor, nickel bead ingredient is Ni >=99.97%, Co ﹤
0.02%, C ﹤ 0.005%, Cu ﹤ 0.002%, Fe ﹤ 0.002%, Pb2+ ﹤ 0.0008%；Or the nickel-contained mixed acid solution and carbonyl that will be adjusted
Base nickel powder is added in nickel powder dissolving tank.
D, adjusting the reaction temperature in reactor or nickel powder dissolving tank is 80 DEG C, and the reaction time is 7 hours, reaction end pH
Value is 2.5, and nickel bead or carbonyl nickel powder, which are dissolved in the sulfuric acid in nickel-contained mixed acid solution, generates nickel sulfate rich solution, in nickel sulfate rich solution
Nickel sulfate content is 356 g/L.
E, by nickel sulfate rich solution filtering and impurity removing, filtered filtrate enters crystallization tank crystallisation by cooling, and crystallization temperature is 20 DEG C,
Nickel sulfate magma is obtained after crystallisation by cooling.
F, wet nickel sulfate hexahydrate crystal is obtained after being centrifugated nickel sulfate magma by centrifugal separator, is obtained after centrifuge separation
Nickel sulfate mother liquor enter mother liquor tank, as in mother liquor return step C reactor or nickel powder dissolving tank recycle.
G, wet nickel sulfate hexahydrate crystal is sent into fluidized bed dryer by auger conveyor and is dried, drying temperature is 40 DEG C, is dried
Nickel sulfate product is obtained after dry, is sent into baling line and is packed.
Nickel sulfate product testing result is as follows:
Claims (5)
1. a kind of method using electro deposited nickel anolyte production nickel sulfate, it is characterised in that method includes the following steps:
A, nitration mixture slot is added according to volume ratio 1:1 in electro deposited nickel anolyte and sulfuric acid and nickel-contained mixed acid solution is made；
B, pure water is added in nickel-contained mixed acid solution, adjusting sulfuric acid concentration in nickel-contained mixed acid solution is 1-1.5M；
C, the nickel-contained mixed acid solution adjusted and nickel bead are added in reactor, or nickel-contained mixed acid solution and carbonyl that will adjust
Nickel powder is added in nickel powder dissolving tank；
D, adjusting the reaction temperature in reactor or nickel powder dissolving tank is 70 DEG C -85 DEG C, and the reaction time is 6-8 hours, and reaction is eventually
Point pH value is 1.5-4.0, and nickel bead or carbonyl nickel powder are dissolved in generation nickel sulfate rich solution, sulfuric acid in the sulfuric acid in nickel-contained mixed acid solution
Nickel sulfate content is 298-356 g/L in nickel rich solution；
E, by nickel sulfate rich solution filtering and impurity removing, filtered filtrate enters crystallization tank crystallisation by cooling and obtains nickel sulfate magma；
F, wet nickel sulfate hexahydrate crystal is obtained after being centrifugated nickel sulfate magma by centrifugal separator；
G, wet nickel sulfate hexahydrate crystal is sent into drier and is dried, obtain nickel sulfate product.
2. a kind of method using electro deposited nickel anolyte production nickel sulfate according to claim 1, it is characterised in that: described
The concentration of sulfuric acid is 93% in step A.
3. a kind of method using electro deposited nickel anolyte production nickel sulfate according to claim 1, it is characterised in that: described
Crystallization temperature is 15 DEG C -25 DEG C in step E.
4. a kind of method using electro deposited nickel anolyte production nickel sulfate according to claim 1, it is characterised in that: described
Reactor or nickel powder dissolving tank after being centrifugated in step F in obtained nickel sulfate mother liquor return step C recycle.
5. a kind of method using electro deposited nickel anolyte production nickel sulfate according to claim 1, it is characterised in that: described
Wet nickel sulfate hexahydrate crystal is sent into fluidized bed dryer by auger conveyor in step G and is dried, drying temperature is 35 DEG C -45 DEG C.
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| CN201910238948.3A CN109809502B (en) | 2019-03-27 | 2019-03-27 | Method for producing nickel sulfate by using electrodeposited nickel anolyte |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111715108A (en) * | 2020-06-16 | 2020-09-29 | 上海大川原德莱因设备工程有限公司 | Stirring hybrid system, drying system and sterilization system |
| WO2023024592A1 (en) * | 2021-08-25 | 2023-03-02 | 广东邦普循环科技有限公司 | Method for preparing nickel sulfate from ferronickel |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756051A (en) * | 2016-12-31 | 2017-05-31 | 山东飞源科技有限公司 | The technique that nickel sulfate is reclaimed from nickel slag |
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2019
- 2019-03-27 CN CN201910238948.3A patent/CN109809502B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756051A (en) * | 2016-12-31 | 2017-05-31 | 山东飞源科技有限公司 | The technique that nickel sulfate is reclaimed from nickel slag |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111715108A (en) * | 2020-06-16 | 2020-09-29 | 上海大川原德莱因设备工程有限公司 | Stirring hybrid system, drying system and sterilization system |
| WO2023024592A1 (en) * | 2021-08-25 | 2023-03-02 | 广东邦普循环科技有限公司 | Method for preparing nickel sulfate from ferronickel |
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| CN109809502B (en) | 2021-06-29 |
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